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Ethyl chloroformate → HCID 20349084、化合物

HRID 1449311
ノート
印刷プレビュー

反応式

HRID 1449311 の反応式
[CH3:1][NH:2][C:3]([N:5]([C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[C:9]([N+:14]([O-:16])=[O:15])[CH:8]=1)O)=[O:4].[OH-].[Na+].Cl[C:20]([O:22]CC)=[O:21]>O1CCOCC1>[N+:14]([C:9]1[CH:8]=[C:7]([N:5]2[C:3](=[O:4])[N:2]([CH3:1])[C:20](=[O:21])[O:22]2)[CH:12]=[CH:11][C:10]=1[CH3:13])([O-:16])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 20349075HCID 20349075、化合物

生成物 1

HCID 20349084HCID 20349084、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

1-Methyl-3-(3'-nitro-4'-methylphenyl)-3-hydroxyurea (11 g; 0.049 mole) was dissolved in dioxane (80 ml.) and mixed with a 2 N aqueous sodium hydroxide (28.5 ml; 0.057 mole). Ethyl chloroformate (5.2 ml; 0.054 mole) was added dropwise at 10°-15° C. with stirring and the stirring continued for about 1/2 hour after the addition was completed. The product which precipitated as formed was removed by filtration, washed with water and dried. This product was recrystallized from methanol and dried under vacuum to yield 2-(3'-nitro-4'-methylphenyl)-4-methyl-1,2,4-oxadiazolidine-3,5-dione as yellow crystals melting 80°-81° C. and having the following elemental analysis as calculated for C10H9N3O5 :

後処理

  1. additionafter the addition
  2. customThe product which precipitated
  3. customas formed
  4. customwas removed by filtration
  5. washwashed with water
  6. customdried
  7. customThis product was recrystallized from methanol
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-0e3864c6585648e9b5c2d60a43e5589e
出典データセット
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04190431

反応ノート

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